The powders of LiFePO4, LiFePO4/C and Li3Fe2(PO4)3 +Fe2O3 have been synthesized by the solid state reaction. The LiFePO4, LiFePO4/C compounds were synthesized in argon atmosphere and Li3Fe2(PO4)3 + Fe2O3 composite was prepared in air. LiFePO4 crystallizes in olivine structure and belongs to the orthorhombic symmetry (space group Pnma). The monoclinic (space group P21/n) Li3Fe2(PO4)3 is of the following lattice parameters — a = 8.5670(6) Å, b = 12.0163(8) Å, c = 8.6148(6) Å, = 79.82 degrees — and well correlates with literature. XRD analysis and Mössbauer spectroscopy also confirms the formation of the -Fe2O3 (hematite) belonging to rhombohedral symmetry (space group R¯3c) of the following lattice parameters: a = 5.0367(4)Å and c =13.7491 (18) Å.Ceramics were sintered for all the measurements.The powder was pressed at 300MPa. LiFePO4/C composite was sintered at 1073K for 1 h in argon atmosphere. The relative densities of LiFePO4/C composite and LiFePO4 ceramics were found to be 73.7% (theoretical density dt = 3.42 g/cm3) and 85.8% (dt = 3.6 g/cm3), respectively. The theoretical densities of Li3Fe2(PO4)3 and Fe2O3 investigated in the present work were found to be 3.127(4) g/cm3 and 5.267(11) g/cm3, respectively. The Archimedes density of the Li3Fe2(PO4)3+Fe2O3 ceramic sample was determined to be 3.06 g/cm3.Impedance spectroscopy of the ceramics has been performed in the frequency range 10 Hz – 10 GHz .